反应详情

A suspension of 2-chloro-4-(p-chloro)phenoxy-2-methyl-3-nitrosobutane (V) (34.20 g) in dry methanol (375 ml) was heated to reflux while ammonia gas was passed through until all the solid dissolved (9.5 hours). Filtration and removal of solvents gave a brown solid, which was largely freed of impurities by washing with benzene. Recrystallisation from isopropanol (a small inorganic residue remained) gave the ketoxime hydrochloride (IV) (19.65 g, yield 54%) as colourless crystals, m.p. 225°-227° (decomp.).

1. temperaturewas heated
2. dissolutiondissolved (9.5 hours)
3. filtrationFiltration and removal of solvents
4. customgave a brown solid, which
5. washby washing with benzene
6. customRecrystallisation from isopropanol (a small inorganic residue